高分辨连续光源原子吸收光谱法测定钒铁中磷  

Determination of phosphorus in ferrovanadium by high resolution continuum source atomic absorption spectrometry

作　　者：王勇 仲利 杨涛 施宗友 

机构地区：[1]攀枝花市产品质量监督检验所国家钒钛制品质量监督检验中心,四川攀枝花617000

出　　处：《冶金分析》2016年第3期1-5,共5页Metallurgical Analysis

摘　　要：由于P的共振线（178nm）位于紫外真空区，直接用火焰原子吸收光谱法进行测定较为困难。而P在适宜比例的乙炔／空气火焰中，可产生一系列PO双原子分子吸收光谱，故可应用连续光源原子吸收光谱法对P进行定量分析。样品用硝酸和盐酸加热溶解完全后，在适宜比例的乙炔／空气火焰中以PO327．04nm为分析线，建立了高分辨连续光源原子吸收光谱法测定钒铁中P的方法。确定了高分辨连续光源原子吸收光谱仪的最佳工作条件为乙炔和空气流速比0．16，燃烧头高度12mm，积分像素点9pixl。实验表明：P质量浓度为5．O～8Omg／L范围内与其吸光度呈良好的线性关系，其线性方程为y=0．0008z＋0．0019，相关系数r为O．9995。方法检出限为1．0mg／L。样品中共存元素的干扰试验表明：基体元素V、Fe对测定P无干扰；Ca、Mg元素对P的测定虽有干扰，但样品中存在的A1因可以与Ca、Mg元素形成较为稳定的CaAl204和MgAl204化合物而消除了其干扰。采用实验方法测定钒铁标准物质和实际样品中P的测定，测得结果与认定值基本一致，相对标准偏差（RSD，n-11）为1．9％～4．4％。Since the resonance line of P(178nm)is in ultraviolet vacuum region,it is difficult to directly determine P by flame atomic absorption spectrometry.However,P could generate a series of PO diatomic molecule absorption spectra in acetylene/air flame with proper proportion,so P could be quantitatively analyzed by continuum source atomic absorption spectrometry.After the sample was fully dissolved with nitric acid and hydrochloric acid by heating,a determination method of P in ferrovanadium by high resolution continuum source atomic absorption spectrometry was established in air-acetylene flame with proper proportion using PO 327.04 nm as analytical line.The optimal working parameters of high resolution continuum source atomic absorption spectrometer were obtained:the flow ratio of acetylene to air was 0.16;the height of combustion head was 12 mm;the integral pixel was 9pixl.The results showed that the mass concentration of P in range of 5.0-80mg/L had good linearity to the absorbance.The linear equation was y=0.000 8 x+0.001 9with correlation coefficient of r=0.999 5.The detection limit of method was 1.0mg/L.The interference test of coexisting elements in sample indicated that the matrix elements including V and Fe had no interference.Ca and Mg in the sample had interference with the determination.However,Al in sample could react with Ca and Mg to form stable CaAl_2O_4 and MgAl_2O_4 compounds,thus eliminating the interference.The proposed method was applied to the determination of P in certified reference material and actual sample of ferrovanadium.The results were basically consistent with the certified values.The relative standard deviations(RSD,n=11)were between 1.9% and 4.4%.

关 键 词：连续光源 原子吸收光谱法 钒铁 磷 分子吸收光谱 

分 类 号：TG115.33[金属学及工艺—物理冶金]